Abstract
Nitrogen adsorption at −195°C serves as routine method for the measurement of surface area of porous materials derived by sol-gel procedures. In a systematic study of the simultaneous effect of the pH and water-silane ratio of the starting solutions of preparation of SiO2 xerogels on their surface areas, it was found that conditions of high acidity and low water/silane ratio result in microporous materials, the surface of which cannot be accessed by N2 at −195°C, within a realistic time scale, but only by CO2 at 0°C. In a typical result for TMOS/water/methanol = 1/2/3 at pH=1.0, the apparent N2-area was zero, while the CO2-area was 414 m2/gr. It is recommended to recheck apparent N2-low surface areas of sol-gel materials by CO2 adsorption. The behavior of pyrene-doped xerogels of this type is in agreement with the structural characterization by adsorption.
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